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Serial capillary gas chromatography/Fourier transform infrared spectrometry/mass spectrometry (GC/IR/MS): qualitative and quantitative analysis of amphetamine, methamphetamine, and related analogues in human urine.
J Anal Toxicol. 1992 Nov-Dec; 16(6):389-97.JA

Abstract

A method using serial capillary gas chromatography/Fourier transform infrared spectroscopy/mass spectrometry (GC/IR/MS) for the analysis of derivatized amphetamine, methamphetamine, and related analogues was developed. The GC/IR/MS was configured and optimized with a Hewlett-Packard (HP) 5890A gas chromatograph with a 12-m x 0.32-mm i.d. HP-5 capillary column serially interfaced through an HP 5965A infrared detector to an HP 5970 mass selective detector with a fused-silica 1.2-m x 0.10-mm i.d. column. Urine samples are extracted and derivatized as heptafluorobutyryl (HFBA) derivatives. For quantitation GC/MS in the selected ion monitoring (SIM) mode was used, with D,L-amphetamine-D5 as the internal standard. Gas chromatography/Fourier transform infrared spectrometry (GC/FT-IR) quantitation uses a selected wavelength chromatogram, spectral subtraction, double internal standard method using both D,L-amphetamine-D5 and 4-phenyl butylamine. Sensitivity for the combined GC/MS and GC/FT-IR system for amphetamine and methamphetamine shows limits of linearity of 100 to 5000 ng/mL, a limit of detection of 25 ng/mL, and a limit of quantitation of 98 ng/mL. The overall recovery for amphetamine and related analogues was greater than 85%. Precision studies for concentrations over the range of 200 to 1500 ng/mL showed coefficients of variations ranging from 2.8 to 13.0%. Correlation studies for quantitative GC/MS SIM and GC/FT-IR are greater than 0.98 for amphetamine, methamphetamine, and related analogues. Each analysis includes GC/MS SIM and GC/FT-IR quantitation, qualitative nonselective full spectra GC/FT-IR, and GC/MS scans of HFBA derivatives cross-referenced with an internal drug library, which provides high confidence and a means for the surveillance of amphetamine-like chemical analogues.

Authors+Show Affiliations

U.S. Army Forensic Tox Drug Test Lab, Fort Meade, MD 20755.No affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

1293407

Citation

Platoff, G E., et al. "Serial Capillary Gas chromatography/Fourier Transform Infrared Spectrometry/mass Spectrometry (GC/IR/MS): Qualitative and Quantitative Analysis of Amphetamine, Methamphetamine, and Related Analogues in Human Urine." Journal of Analytical Toxicology, vol. 16, no. 6, 1992, pp. 389-97.
Platoff GE, Hill DW, Koch TR, et al. Serial capillary gas chromatography/Fourier transform infrared spectrometry/mass spectrometry (GC/IR/MS): qualitative and quantitative analysis of amphetamine, methamphetamine, and related analogues in human urine. J Anal Toxicol. 1992;16(6):389-97.
Platoff, G. E., Hill, D. W., Koch, T. R., & Caplan, Y. H. (1992). Serial capillary gas chromatography/Fourier transform infrared spectrometry/mass spectrometry (GC/IR/MS): qualitative and quantitative analysis of amphetamine, methamphetamine, and related analogues in human urine. Journal of Analytical Toxicology, 16(6), 389-97.
Platoff GE, et al. Serial Capillary Gas chromatography/Fourier Transform Infrared Spectrometry/mass Spectrometry (GC/IR/MS): Qualitative and Quantitative Analysis of Amphetamine, Methamphetamine, and Related Analogues in Human Urine. J Anal Toxicol. 1992 Nov-Dec;16(6):389-97. PubMed PMID: 1293407.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Serial capillary gas chromatography/Fourier transform infrared spectrometry/mass spectrometry (GC/IR/MS): qualitative and quantitative analysis of amphetamine, methamphetamine, and related analogues in human urine. AU - Platoff,G E,Jr AU - Hill,D W, AU - Koch,T R, AU - Caplan,Y H, PY - 1992/11/11/pubmed PY - 2001/3/28/medline PY - 1992/11/11/entrez SP - 389 EP - 97 JF - Journal of analytical toxicology JO - J Anal Toxicol VL - 16 IS - 6 N2 - A method using serial capillary gas chromatography/Fourier transform infrared spectroscopy/mass spectrometry (GC/IR/MS) for the analysis of derivatized amphetamine, methamphetamine, and related analogues was developed. The GC/IR/MS was configured and optimized with a Hewlett-Packard (HP) 5890A gas chromatograph with a 12-m x 0.32-mm i.d. HP-5 capillary column serially interfaced through an HP 5965A infrared detector to an HP 5970 mass selective detector with a fused-silica 1.2-m x 0.10-mm i.d. column. Urine samples are extracted and derivatized as heptafluorobutyryl (HFBA) derivatives. For quantitation GC/MS in the selected ion monitoring (SIM) mode was used, with D,L-amphetamine-D5 as the internal standard. Gas chromatography/Fourier transform infrared spectrometry (GC/FT-IR) quantitation uses a selected wavelength chromatogram, spectral subtraction, double internal standard method using both D,L-amphetamine-D5 and 4-phenyl butylamine. Sensitivity for the combined GC/MS and GC/FT-IR system for amphetamine and methamphetamine shows limits of linearity of 100 to 5000 ng/mL, a limit of detection of 25 ng/mL, and a limit of quantitation of 98 ng/mL. The overall recovery for amphetamine and related analogues was greater than 85%. Precision studies for concentrations over the range of 200 to 1500 ng/mL showed coefficients of variations ranging from 2.8 to 13.0%. Correlation studies for quantitative GC/MS SIM and GC/FT-IR are greater than 0.98 for amphetamine, methamphetamine, and related analogues. Each analysis includes GC/MS SIM and GC/FT-IR quantitation, qualitative nonselective full spectra GC/FT-IR, and GC/MS scans of HFBA derivatives cross-referenced with an internal drug library, which provides high confidence and a means for the surveillance of amphetamine-like chemical analogues. SN - 0146-4760 UR - https://www.unboundmedicine.com/medline/citation/1293407/Serial_capillary_gas_chromatography/Fourier_transform_infrared_spectrometry/mass_spectrometry__GC/IR/MS_:_qualitative_and_quantitative_analysis_of_amphetamine_methamphetamine_and_related_analogues_in_human_urine_ L2 - https://academic.oup.com/jat/article-lookup/doi/10.1093/jat/16.6.389 DB - PRIME DP - Unbound Medicine ER -